Tall Oil Fatty Acids, compounds with 2-(2-aminoethoxy) ethanol

Stability in organic solvents and identity of relevant degradation products

Link to relevant study record(s)

Reference

Endpoint:

stability in organic solvents and identity of relevant degradation products

Type of information:

experimental study

Adequacy of study:

key study

Study period:

18 August 2015 to 06 November 2015

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

study well documented, meets generally accepted scientific principles, acceptable for assessment

Qualifier:

no guideline available

Principles of method if other than guideline:

HPLC method using UV absorbance detection at a wavelength of 280 nm for determination of test material concentration and stability in peanut oil formulations.

GLP compliance:

yes

Test substance stable:

yes

- Under the described chromatographic conditions, the retention time of the test item was approximately 4.8 minutes.

- The total analysis time for each run was 10.0 minutes.

- Assay specificity/selectivity was confirmed when HPLC/UV analysis of processed vehicle samples revealed no significant peaks (with S/N > 10) at or near the retention time for the test item.

- The post-storage test substance concentrations ranged from 95.4 % to 107 % of the pre-storage values.

- For a nominal concentration of 1 mg/mL, mean concentration at time zero was determined to be 0.846 mg/mL (97.8 % of pre-storage value) after 6 days at room temperature.

- For a nominal concentration of 1 mg/mL, mean concentration at time zero was determined to be 0.847 mg/mL (97.9 % of pre-storage value) after 12 days at room temperature.

- For a nominal concentration of 220 mg/mL, mean concentration at time zero was determined to be 253 mg/mL (107 % of pre-storage value) after 6 days at room temperature.

- For a nominal concentration of 220 mg/mL, mean concentration at time zero was determined to be 226 mg/mL (95.4 % of pre-storage value) after 12 days at room temperature.

Conclusions:

Formulations prepared at target test substance concentrations of 1 and 220 mg/mL met the protocol-specified requirement for homogeneity and for storage, re-suspension homogeneity and stability after 6 and 12 days storage at room temperature.

Executive summary:

METHOD

Test item concentration from 1.00 to 220 mg/mL in peanut oil was determined using an HPLC method and UV absorbance at a wavelength of 280 nm. Test item stability was also assessed in a QC stock solutions stored at room temperature for 1 and 6 days, in primary dilutions stored at room temperature for 6 days, and in calibration standards and processed QC samples stored at room temperature for 5 days. Test substance homogeneity was assessed and re-suspension homogeneity and stabilty were assessed after 6 and 12 days of room temperature storage in formulations prepared at target concentrations of 1 and 220 mg/mL test item.

RESULTS

The test material assay procedure was validated in this study with 3 validation sessions. Quantitation was performed using calibration standards ranging in test item concentration from 100 to 500 μg/mL. The mean back-calculated standard concentrations had inter-session variability ranging from 0.16 % to 0.96 % Relative Standard Deviation (RSD) and % Relative Error (RE) ranging from -0.11 % to 0.14 %, which met the protocol-specified acceptance criteria for calibration standards, i.e., RSD ≤10% (≤15% at the lowest concentration) and %RE within ± 10% (± 15% at the lowest concentration). Assay precision and accuracy were verified by the analysis of QC samples prepared at nominal concentrations of 1.00, 40.0, and 220 mg/m test material. The mean calculated QC concentrations had inter-session variability (precision) ranging from 1.8 % to 2.4 % RSD and %RE (accuracy) ranging from -14 % to 0.27 %, which met the protocol-specified acceptance criteria for precision and accuracy, i.e., RSD ≤ 15% and %RE within ± 15%.

The test substance met the protocol-specified acceptance criteria for stability in a QC stock solution stored at room temperature for 1 day, in primary dilutions stored at room temperature for 6 days, and in calibration standards and processed QC samples stored at room temperature for 5 days (post-storage concentration was not < 90 % of the pre-storage value or the theoretical value).

The results of the test substance homogeneity assessment in formulations prepared at target concentrations of 1 and 220 mg/mL test item met the protocol-specified acceptance criteria ((RSD for the mean concentration was ≤ 10 % at a concentration within the acceptable limits of 85 % to 115 % of target).

Assessment of test substance re-suspension homogeneity and stability met the protocol-specified acceptance criteria in formulations prepared at target concentrations of 1 and 220 mg/mL test item and stored at room temperature for 6 and 12 days (RSD for the mean concentration was ≤ 10 % and post-storage concentration was not < 90 % of the pre-storage value or the theoretical value.

CONCLUSION

Formulations prepared at target test substance concentrations of 1 and 220 mg/mL met the protocol-specified requirement for homogeneity and for storage, re-suspension homogeneity and stability after 6 and 12 days storage at room temperature.

Description of key information

The post-storage test substance concentrations of formulations prepared at target test substance concentrations of 1 and 220 mg/mL in peanut oil ranged from 95.4 % to 107 % of the pre-storage values. As such, the test item met the protocol-specified requirement for homogeneity and for storage, re-suspension homogeneity and stability after 6 and 12 days storage at room temperature.

Additional information

No additional data.